CN114907495A - Efficient extraction process of hericium erinaceus polysaccharide - Google Patents

Efficient extraction process of hericium erinaceus polysaccharide Download PDF

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CN114907495A
CN114907495A CN202210599680.8A CN202210599680A CN114907495A CN 114907495 A CN114907495 A CN 114907495A CN 202210599680 A CN202210599680 A CN 202210599680A CN 114907495 A CN114907495 A CN 114907495A
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hericium erinaceus
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erinaceus powder
polysaccharide
extraction process
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CN114907495B (en
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王春艳
张英波
董玉玮
许海旭
李文
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China Zhongjian An Hangzhou Molecular Medicine Technology Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

The invention relates to the technical field of hericium erinaceus processing, and particularly discloses a high-efficiency extraction process of hericium erinaceus polysaccharide, which comprises the following steps: (1) soaking Hericium erinaceus powder in clear water to make Hericium erinaceus cells fully absorb water to obtain imbibition Hericium erinaceus powder. (2) And (3) steaming the imbibed hericium erinaceus powder in a heating and pressurizing environment by using carbon dioxide and water vapor to obtain the pretreated hericium erinaceus powder. (3) Freezing the pretreated hericium erinaceus powder to freeze liquid water absorbed in hericium erinaceus cells; and then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition to obtain the wall-broken hericium erinaceus powder. (4) Extracting the wall-broken hericium erinaceus powder with hot water, and performing separation and purification procedures to obtain the hericium erinaceus polysaccharide extract. The invention adopts the mode of firstly carrying out crisping treatment on the cell wall of the hericium erinaceus and then carrying out impact wall breaking on the crisped cell wall from the inside of the cell by utilizing freezing and vacuum microwave heat shock, thereby obtaining good wall breaking effect.

Description

Efficient extraction process of hericium erinaceus polysaccharide
Technical Field
The invention relates to the technical field of hericium erinaceus processing, and particularly relates to a high-efficiency extraction process of hericium erinaceus polysaccharide.
Background
Hericium erinaceus is also called Leonurus japonicus, Hericium erinaceus, etc., and is called Hericium erinaceus because of the head of the externally-grown monkey. The hericium erinaceus has the effects of enhancing immunity, reducing blood fat and cholesterol, resisting aging, resisting cancer and the like, and particularly polysaccharides contained in the hericium erinaceus have the effects of preventing the regeneration of cancer cells and inhibiting the synthesis of genetic materials in the cancer cells; but also is helpful for promoting digestion and repairing damaged cells, thereby achieving the effect of protecting intestines and stomach.
The hericium erinaceus polysaccharide is an active ingredient extracted from hericium erinaceus, and the current extraction method mainly comprises hot water extraction, acid extraction, alkali extraction, enzyme extraction and the like. Since the hericium erinaceus cells have a firm cell wall structure and polysaccharide substances are contained in the hericium erinaceus cells to hinder extraction, generally, in order to achieve a higher extraction rate of the polysaccharide, the hericium erinaceus is subjected to a wall-breaking treatment before extraction to expose the polysaccharide substances therein as sufficiently as possible. However, the current better wall breaking effect needs a special instrument, the cost is high, the preparation is difficult in a common laboratory, the common mechanical wall breaking effect is not ideal, the method for breaking the wall by enzyme treatment is not easy to control, and the damage to the polysaccharide is easily caused.
Disclosure of Invention
Aiming at the problems, the invention provides the high-efficiency extraction process of the hericium erinaceus polysaccharide, which has strong operability and good wall breaking effect. To achieve the above object, the present invention specifically provides the following.
A high-efficiency extraction process of hericium erinaceus polysaccharide comprises the following steps:
(1) soaking Hericium erinaceus powder in clear water to make Hericium erinaceus cells fully absorb water to obtain imbibition Hericium erinaceus powder for use.
(2) And (3) steaming the imbibed hericium erinaceus powder in a heating and pressurizing environment by using carbon dioxide and water vapor to obtain pretreated hericium erinaceus powder for later use.
(3) Freezing the pretreated hericium erinaceus powder to freeze liquid water absorbed in hericium erinaceus cells; and then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition to obtain the wall-broken hericium erinaceus powder.
(4) Extracting the wall-broken hericium erinaceus powder with hot water, and performing separation and purification procedures to obtain the hericium erinaceus polysaccharide extract.
Further, in the step (1), the soaking is not less than 2 hours, preferably 3 to 3.5 hours, and more preferably, the soaking is performed by using low-temperature water with the temperature not higher than 5 ℃.
Further, in the step (2), the volume ratio of the carbon dioxide to the water vapor is 1: 1.7-2.5, wherein the ratio of the imbibition hericium erinaceus powder to the gas is 1 g: 50-80 ml, wherein the gas is the sum of carbon dioxide and water vapor.
So that the carbon dioxide is dissolved in the water vapor and hydrogen ions are ionized to carry out the crisping treatment on the cell walls of the hericium erinaceus powder.
Further, in the step (2), the heating temperature is 105-110 ℃. Under the heating and pressurizing conditions, the water vapor condensation is avoided, and meanwhile, the effect of crisping the cell walls of the hericium erinaceus powder is promoted.
Further, in the step (2), the steam curing time is 25-40 min, and the aim of crisping the cell wall of the hericium erinaceus and reducing the strength of the cell wall can be achieved by steam curing the hericium erinaceus powder in a special high-temperature and high-pressure environment created by carbon dioxide and water vapor.
Further, in the step (3), the pretreated hericium erinaceus powder is frozen to-10 to-15 ℃, so that liquid water absorbed in hericium erinaceus cells is quickly frozen.
Further, in the step (3), the temperature of the microwave thermal shock treatment is 50-70 ℃, the time is 3-5 min, and the vacuum degree is-0.2-0.1 MPa. The microwave heat shock under the vacuum condition can lead the ice in the hericium erinaceus cells to be quickly gasified, impact and expand the crisp hericium erinaceus cell walls.
Further, in the step (4), the hot water leaching temperature is 50-65 ℃, and the leaching time is 45-60 min. The polysaccharide and other substances in the hericium erinaceus wall-broken cells are fully dissolved in hot water through hot water extraction, so that the primary extraction of the hericium erinaceus polysaccharide is realized.
Further, in the step (4), the separation and purification process includes: and (4) sequentially carrying out decoloring, alcohol precipitation, solid-liquid separation and vacuum drying on the leaching solution.
Further, the decoloring treatment is realized by any one of activated carbon and hydrogen peroxide.
Further, the alcohol precipitation treatment is realized by using ethanol with the concentration of more than 95 percent, which is obtained by decoloring and has more than four times of the volume of a leaching liquor. Because the hericium erinaceus polysaccharide is insoluble in ethanol, the polysaccharide can be separated out in a precipitate form after the ethanol is added into the leaching liquor, and the precipitate is dried in vacuum at 40-50 ℃ after solid-liquid separation to obtain the hericium erinaceus polysaccharide extract.
Compared with the prior art, the invention has the following beneficial effects: as described above, the cell wall of hericium erinaceus is subjected to a wall-breaking treatment, which is important for extracting polysaccharide substances from the cell wall, but some of the current wall-breaking techniques have various disadvantages. Therefore, the method adopts the mode of firstly carrying out crisping treatment on the cell wall of the hericium erinaceus in the special environment created by carbon dioxide and high-temperature steam and then carrying out impact wall breaking on the crisped cell wall from the inside of the cell by utilizing freezing and vacuum microwave heat shock, and not only has strong operability, but also has good wall breaking effect. The reason for this is that: firstly, weak acid mist formed after mixing carbon dioxide and high-temperature steam is contacted with cell walls, then hydrogen ions enter the cell walls, the cell walls are gradually crisped under the action of the hydrogen ions, the crisping has the advantages that the strength of the cell walls can be effectively reduced, and the cell walls are convenient to break. Based on the research, the invention adopts the mode of crisping the hericium erinaceus cell wall before wall breaking, so that the barrier of firm cell wall to the wall breaking is reduced. Meanwhile, the loss of water absorbed in the hericium erinaceus cells can be prevented by adopting a high-humidity environment of carbon dioxide and water vapor, the cells are ensured to be in a water-swelling state, and necessary conditions and foundations are provided for subsequent wall breaking. On the basis, the obtained pretreated hericium erinaceus powder has the characteristics that the cell walls are crisp and are in an imbibition state, and good necessary conditions and basis are provided for subsequent wall breaking. Furthermore, the invention firstly freezes the preprocessed hericium erinaceus powder, and then carries out the wall breaking in a microwave heat shock mode under the vacuum condition, because the liquid in the cells of the preprocessed hericium erinaceus powder after being quickly frozen freezes and expands in volume, the cell walls are extruded from inside to outside, because the strength of the cell walls is obviously reduced after being subjected to the crisping treatment, cracks are easy to appear under extrusion, the cracks become the basis of final wall breaking, when the hericium erinaceus is processed by microwaves under the vacuum condition, the ice in the cells is quickly sublimated into high-pressure steam under the microwave and vacuum actions, and the instant gasification of the ice causes huge pressure difference inside and outside the cells, the cracks on the cell walls rapidly expand and extend under the strong impact of the steam inside the cells, the wall breaking degree of the cell walls is improved, and the efficient extraction of polysaccharide substances in the hericium erinaceus is convenient, improve the extraction rate of polysaccharide substances.
Detailed Description
It is to be understood that all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, unless otherwise defined. The reagents or starting materials used in the present invention can be purchased from conventional sources, and unless otherwise specified, the reagents or starting materials used in the present invention can be used in a conventional manner in the art or in accordance with the product specifications.
In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only. The invention will be further illustrated with reference to the following specific examples.
Example 1
A high-efficiency extraction process of hericium erinaceus polysaccharide comprises the following steps:
(1) pulverizing dried Hericium erinaceus, and sieving with 100 mesh sieve (the residue is less than or equal to 5%) to obtain Hericium erinaceus powder.
(2) And (2) soaking the hericium erinaceus powder obtained in the step (1) in deionized water at the temperature of 3 ℃ and stirring to fully mix the hericium erinaceus powder and the deionized water, and then soaking for 3 hours to fully absorb water in hericium erinaceus cells to obtain the imbibition hericium erinaceus powder.
(3) Placing the imbibition hericium erinaceus powder obtained in the step (2) in a reaction kettle, and then mixing the carbon dioxide and the water vapor according to a volume ratio of 1: 2, introducing carbon dioxide and water vapor into the reaction kettle, wherein the ratio of the imbibed hericium erinaceus powder to the gas (carbon dioxide and water vapor) is 1 g: 80ml, heating in water bath, maintaining the temperature at 110 deg.C for 35min, and steaming at high temperature and high pressure to obtain pretreated Hericium erinaceus powder.
(4) Taking out the pretreated hericium erinaceus powder prepared in the step (3), and then putting the pretreated hericium erinaceus powder into a refrigerator to be frozen to-15 ℃; and then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition, wherein the temperature of the heat shock treatment by microwaves is 65 ℃, the time is 5min, and the vacuum degree is-0.1 MPa, so that the wall-broken hericium erinaceus powder is obtained.
(5) Taking 100g of the broken hericium erinaceus powder prepared in the step (4), and mixing the materials in a proportion of 1 g: adding the wall-broken hericium erinaceus powder into hot water of 60 ℃ at a proportion of 50ml, uniformly stirring, carrying out ultrasonic treatment at the temperature for 50min, filtering the leaching solution after completion, adding activated carbon into the collected filtrate for decolorization, then adding ethanol (the mass concentration is 95%) with the volume being four times of that of the filtrate into the decolorized solution, standing and precipitating for 20h, then carrying out centrifugal separation on the precipitate, and carrying out vacuum drying at 40 ℃ to obtain the hericium erinaceus polysaccharide extract.
Example 2
A high-efficiency extraction process of hericium erinaceus polysaccharide comprises the following steps:
(1) pulverizing dried Hericium erinaceus, and sieving with 100 mesh sieve (the residue is less than or equal to 5%) to obtain Hericium erinaceus powder.
(2) And (2) soaking the hericium erinaceus powder obtained in the step (1) in deionized water at the temperature of 5 ℃ and stirring to fully mix the hericium erinaceus powder and the deionized water, and then soaking for 3.5 hours to fully absorb water in hericium erinaceus cells to obtain the imbibition hericium erinaceus powder.
(3) Placing the imbibition hericium erinaceus powder obtained in the step (2) in a reaction kettle, and then mixing the carbon dioxide and the water vapor according to a volume ratio of 1: 1.7, introducing carbon dioxide and water vapor into the reaction kettle, wherein the ratio of the imbibed hericium erinaceus powder to the gas (carbon dioxide + water vapor) is 1 g: 60ml, then heating in water bath and maintaining the temperature at 110 ℃ for 30min, and steaming the imbibed hericium erinaceus powder at high temperature and high pressure to obtain pretreated hericium erinaceus powder for later use.
(4) Taking out the pretreated hericium erinaceus powder prepared in the step (3), and then putting the pretreated hericium erinaceus powder into a refrigerator to be frozen to-15 ℃; and then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition, wherein the temperature of the heat shock treatment by microwaves is 60 ℃, the time is 4min, and the vacuum degree is-0.1 MPa, so that the wall-broken hericium erinaceus powder is obtained.
(5) Taking 100g of the wall-broken hericium erinaceus powder prepared in the step (4), and mixing the powder according to the weight ratio of 1 g: adding 50ml of the wall-broken hericium erinaceus powder into hot water at 65 ℃, uniformly stirring, performing ultrasonic treatment at the temperature for 45min, filtering the leaching solution, adding activated carbon into the collected filtrate for decoloring, adding ethanol with the volume being five times that of the filtrate (the mass concentration is 95%) into the decoloring solution, standing and precipitating for 20h, then performing centrifugal separation to obtain precipitate, and performing vacuum drying at 40 ℃ to obtain the hericium erinaceus polysaccharide extract.
Example 3
A high-efficiency extraction process of hericium erinaceus polysaccharide comprises the following steps:
(1) pulverizing dried Hericium erinaceus, and sieving with 100 mesh sieve (the residue is less than or equal to 5%) to obtain Hericium erinaceus powder.
(2) And (2) soaking the hericium erinaceus powder obtained in the step (1) in deionized water at the temperature of 5 ℃ and stirring to fully mix the hericium erinaceus powder and the deionized water, and then soaking for 2 hours to fully absorb water in hericium erinaceus cells to obtain the imbibition hericium erinaceus powder.
(3) Placing the imbibition hericium erinaceus powder obtained in the step (2) in a reaction kettle, and then mixing the carbon dioxide and the water vapor according to a volume ratio of 1: 2.2, introducing carbon dioxide and water vapor into the reaction kettle, wherein the ratio of the imbibed hericium erinaceus powder to the gas (carbon dioxide + water vapor) is 1 g: 50ml, heating in water bath, maintaining the temperature at 105 deg.C for 40min, and steaming at high temperature and high pressure to obtain pretreated Hericium erinaceus powder.
(4) Taking out the pretreated hericium erinaceus powder prepared in the step (3), and then putting the pretreated hericium erinaceus powder into a refrigerator to be frozen to-10 ℃; and then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition, wherein the temperature of the heat shock treatment by microwaves is 50 ℃, the time is 5min, and the vacuum degree is-0.2 MPa, so that the wall-broken hericium erinaceus powder is obtained.
(5) Taking 100g of the wall-broken hericium erinaceus powder prepared in the step (4), and mixing the powder according to the weight ratio of 1 g: adding the wall-broken hericium erinaceus powder into 50ml of hot water at the temperature of 50 ℃, uniformly stirring, carrying out ultrasonic treatment at the temperature for 60min, filtering the leaching liquor after completion, adding activated carbon into the collected filtrate for decolorization, then adding ethanol with the volume being five times that of the filtrate (the mass concentration is 95%) into the decolorized solution, standing and precipitating for 20h, then carrying out centrifugal separation on the precipitate, and carrying out vacuum drying at the temperature of 40 ℃ to obtain the hericium erinaceus polysaccharide extract.
Example 4
A high-efficiency extraction process of hericium erinaceus polysaccharide comprises the following steps:
(1) pulverizing dried Hericium erinaceus, and sieving with 100 mesh sieve (the residue is less than or equal to 5%) to obtain Hericium erinaceus powder.
(2) And (2) soaking the hericium erinaceus powder obtained in the step (1) in deionized water at the temperature of 2 ℃ and stirring to fully mix the hericium erinaceus powder and the deionized water, and then soaking for 3 hours to fully absorb water in hericium erinaceus cells to obtain the imbibition hericium erinaceus powder.
(3) Placing the imbibition hericium erinaceus powder obtained in the step (2) in a reaction kettle, and then mixing the carbon dioxide and the water vapor according to a volume ratio of 1: 2.5, introducing carbon dioxide and water vapor into the reaction kettle, wherein the ratio of the imbibed hericium erinaceus powder to the gas (carbon dioxide + water vapor) is 1 g: 70ml, then heating in water bath and maintaining the temperature at 110 ℃ for 25min, and steaming the imbibed hericium erinaceus powder at high temperature and high pressure to obtain pretreated hericium erinaceus powder for later use.
(4) Taking out the pretreated hericium erinaceus powder prepared in the step (3), and then putting the pretreated hericium erinaceus powder into a refrigerator to be frozen to-12 ℃; and then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition, wherein the temperature of the heat shock treatment by microwaves is 70 ℃, the time is 3min, and the vacuum degree is-0.2 MPa, so that the wall-broken hericium erinaceus powder is obtained.
(5) Taking 100g of the wall-broken hericium erinaceus powder prepared in the step (4), and mixing the powder according to the weight ratio of 1 g: adding the wall-broken hericium erinaceus powder into hot water of 60 ℃ at a proportion of 50ml, uniformly stirring, carrying out ultrasonic treatment at the temperature for 55min, filtering the leaching solution after completion, adding activated carbon into the collected filtrate for decolorization, then adding ethanol (the mass concentration is 95%) with the volume being five times of that of the filtrate into the decolorized solution, standing and precipitating for 20h, then carrying out centrifugal separation on the precipitate, and carrying out vacuum drying at 40 ℃ to obtain the hericium erinaceus polysaccharide extract.
Example 5
A high-efficiency extraction process of hericium erinaceus polysaccharide comprises the following steps:
(1) pulverizing dried Hericium erinaceus, and sieving with 100 mesh sieve (the residue is less than or equal to 5%) to obtain Hericium erinaceus powder.
(2) Putting the hericium erinaceus powder obtained in the step (1) into a reaction kettle, and then mixing the hericium erinaceus powder with water vapor according to the volume ratio of carbon dioxide to water vapor of 1: 2, introducing carbon dioxide and water vapor into the reaction kettle, wherein the ratio of the imbibed hericium erinaceus powder to the gas (carbon dioxide and water vapor) is 1 g: 80ml, heating in water bath, maintaining the temperature at 110 deg.C for 35min, and steaming at high temperature and high pressure to obtain pretreated Hericium erinaceus powder.
(3) Taking out the preprocessed hericium erinaceus powder prepared in the step (2), and then putting the hericium erinaceus powder in a refrigerator to be frozen to-15 ℃; and then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition, wherein the temperature of the heat shock treatment by microwaves is 65 ℃, the time is 5min, and the vacuum degree is-0.1 MPa, so as to obtain the wall-broken hericium erinaceus powder.
(4) Taking 100g of the broken hericium erinaceus powder prepared in the step (3), and mixing the materials in a proportion of 1 g: adding the wall-broken hericium erinaceus powder into hot water of 60 ℃ at a proportion of 50ml, uniformly stirring, carrying out ultrasonic treatment at the temperature for 50min, filtering the leaching solution after completion, adding activated carbon into the collected filtrate for decolorization, then adding ethanol (the mass concentration is 95%) with the volume being four times of that of the filtrate into the decolorized solution, standing and precipitating for 20h, then carrying out centrifugal separation on the precipitate, and carrying out vacuum drying at 40 ℃ to obtain the hericium erinaceus polysaccharide extract.
Example 6
A high-efficiency extraction process of hericium erinaceus polysaccharide comprises the following steps:
(1) pulverizing dried Hericium erinaceus, and sieving with 100 mesh sieve (the residue is less than or equal to 5%) to obtain Hericium erinaceus powder.
(2) And (2) soaking the hericium erinaceus powder obtained in the step (1) in deionized water at the temperature of 3 ℃ and stirring to fully mix the hericium erinaceus powder and the deionized water, and then soaking for 3 hours to fully absorb water in hericium erinaceus cells to obtain the imbibition hericium erinaceus powder.
(3) Taking out the imbibition hericium erinaceus powder obtained in the step (2), and then placing the imbibition hericium erinaceus powder in a refrigerator to be frozen to-15 ℃; and then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition, wherein the temperature of the heat shock treatment by microwaves is 65 ℃, the time is 5min, and the vacuum degree is-0.1 MPa, so that the wall-broken hericium erinaceus powder is obtained.
(4) Taking 100g of the broken hericium erinaceus powder prepared in the step (3), and mixing the materials in a proportion of 1 g: adding the wall-broken hericium erinaceus powder into hot water of 60 ℃ at a proportion of 50ml, uniformly stirring, carrying out ultrasonic treatment at the temperature for 50min, filtering the leaching solution after completion, adding activated carbon into the collected filtrate for decolorization, then adding ethanol (the mass concentration is 95%) with the volume being four times of that of the filtrate into the decolorized solution, standing and precipitating for 20h, then carrying out centrifugal separation on the precipitate, and carrying out vacuum drying at 40 ℃ to obtain the hericium erinaceus polysaccharide extract.
Example 7
A high-efficiency extraction process of hericium erinaceus polysaccharide comprises the following steps:
(1) pulverizing dried Hericium erinaceus, and sieving with 100 mesh sieve (the residue on sieve is less than or equal to 5%) to obtain Hericium erinaceus powder.
(2) And (2) soaking the hericium erinaceus powder obtained in the step (1) in deionized water at the temperature of 3 ℃ and stirring to fully mix the hericium erinaceus powder and the deionized water, and then soaking for 3 hours to fully absorb water in hericium erinaceus cells to obtain the imbibition hericium erinaceus powder.
(3) Placing the imbibition hericium erinaceus powder obtained in the step (2) in a reaction kettle, and then mixing the carbon dioxide and the water vapor according to a volume ratio of 1: 2, introducing carbon dioxide and water vapor into the reaction kettle, wherein the ratio of the imbibed hericium erinaceus powder to the gas (carbon dioxide and water vapor) is 1 g: 80ml, heating in water bath, maintaining the temperature at 110 deg.C for 35min, and steaming at high temperature and high pressure to obtain pretreated Hericium erinaceus powder.
(4) Taking out the pretreated hericium erinaceus powder prepared in the step (3), and then putting the pretreated hericium erinaceus powder into a refrigerator to be frozen to-15 ℃; heating the frozen Hericium erinaceus powder in water bath to 65 deg.C, and keeping the temperature for 5min to obtain wall-broken Hericium erinaceus powder.
(5) Taking 100g of the wall-broken hericium erinaceus powder prepared in the step (4), and mixing the powder according to the weight ratio of 1 g: adding the wall-broken hericium erinaceus powder into hot water of 60 ℃ at a proportion of 50ml, uniformly stirring, carrying out ultrasonic treatment at the temperature for 50min, filtering the leaching solution after completion, adding activated carbon into the collected filtrate for decolorization, then adding ethanol (the mass concentration is 95%) with the volume being four times of that of the filtrate into the decolorized solution, standing and precipitating for 20h, then carrying out centrifugal separation on the precipitate, and carrying out vacuum drying at 40 ℃ to obtain the hericium erinaceus polysaccharide extract.
Example 8
A high-efficiency extraction process of hericium erinaceus polysaccharide comprises the following steps:
(1) pulverizing dried Hericium erinaceus, and sieving with 100 mesh sieve (the residue is less than or equal to 5%) to obtain Hericium erinaceus powder.
(2) And (2) soaking the hericium erinaceus powder obtained in the step (1) into deionized water at the temperature of 3 ℃ and stirring to fully mix the hericium erinaceus powder and the deionized water, and then soaking for 3 hours to fully absorb water in hericium erinaceus cells to obtain the imbibition hericium erinaceus powder.
(3) Placing the imbibition hericium erinaceus powder obtained in the step (2) in a reaction kettle, and mixing the imbibition hericium erinaceus powder with carbon dioxide in an amount of 1 g: introducing carbon dioxide into the reaction kettle in a proportion of 80ml, heating in water bath, maintaining the temperature at 110 ℃ for 35min, and steaming the imbibed hericium erinaceus powder at high temperature and high pressure to obtain pretreated hericium erinaceus powder for later use.
(4) Taking out the pretreated hericium erinaceus powder prepared in the step (3), and then putting the pretreated hericium erinaceus powder into a refrigerator to be frozen to-15 ℃; and then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition, wherein the temperature of the heat shock treatment by microwaves is 65 ℃, the time is 5min, and the vacuum degree is-0.1 MPa, so that the wall-broken hericium erinaceus powder is obtained.
(5) Taking 100g of the wall-broken hericium erinaceus powder prepared in the step (4), and mixing the powder according to the weight ratio of 1 g: adding the wall-broken hericium erinaceus powder into hot water of 60 ℃ at a proportion of 50ml, uniformly stirring, carrying out ultrasonic treatment at the temperature for 50min, filtering the leaching solution after completion, adding activated carbon into the collected filtrate for decolorization, then adding ethanol (the mass concentration is 95%) with the volume being four times of that of the filtrate into the decolorized solution, standing and precipitating for 20h, then carrying out centrifugal separation on the precipitate, and carrying out vacuum drying at 40 ℃ to obtain the hericium erinaceus polysaccharide extract.
Example 9
A high-efficiency extraction process of hericium erinaceus polysaccharide comprises the following steps:
(1) pulverizing dried Hericium erinaceus, and sieving with 100 mesh sieve (the residue is less than or equal to 5%) to obtain Hericium erinaceus powder.
(2) And (2) soaking the hericium erinaceus powder obtained in the step (1) in deionized water at the temperature of 3 ℃ and stirring to fully mix the hericium erinaceus powder and the deionized water, and then soaking for 3 hours to fully absorb water in hericium erinaceus cells to obtain the imbibition hericium erinaceus powder.
(3) Placing the imbibition hericium erinaceus powder obtained in the step (2) in a reaction kettle, and mixing the imbibition hericium erinaceus powder with water vapor in an amount of 1 g: adding 80ml of water vapor into a reaction kettle, heating in a water bath, maintaining the temperature at 110 ℃ for 35min, and steaming the imbibed hericium erinaceus powder at high temperature and high pressure to obtain pretreated hericium erinaceus powder for later use.
(4) Taking out the pretreated hericium erinaceus powder prepared in the step (3), and then putting the pretreated hericium erinaceus powder into a refrigerator to be frozen to-15 ℃; and then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition, wherein the temperature of the heat shock treatment by microwaves is 65 ℃, the time is 5min, and the vacuum degree is-0.1 MPa, so as to obtain the wall-broken hericium erinaceus powder.
(5) Taking 100g of the broken hericium erinaceus powder prepared in the step (4), and mixing the materials in a proportion of 1 g: adding the wall-broken hericium erinaceus powder into hot water of 60 ℃ at a proportion of 50ml, uniformly stirring, carrying out ultrasonic treatment at the temperature for 50min, filtering the leaching solution after completion, adding activated carbon into the collected filtrate for decolorization, then adding ethanol (the mass concentration is 95%) with the volume being four times of that of the filtrate into the decolorized solution, standing and precipitating for 20h, then carrying out centrifugal separation on the precipitate, and carrying out vacuum drying at 40 ℃ to obtain the hericium erinaceus polysaccharide extract.
The hericium erinaceus spore powder wall breaking rate of each example is measured, and the hericium erinaceus polysaccharide extraction rate of each example is measured by a phenol-sulfuric acid method, and the results are shown in table 1.
TABLE 1
Example number 1 2 3 4 5 6 7 8 9
Wall breaking rate/%) 97.62 94.37 96.19 98.74 46.88 41.48 63.81 75.44 68.27
Yield/% 21.16 17.55 19.23 21.91 7.29 5.33 9.67 11.92 8.83
From the result of last table can see out, through adopting earlier to crisp the cell wall of hericium erinaceus in the special environment that carbon dioxide and high temperature vapor created, then utilize freezing and the mode that the cell wall is strikeed to crisp from the cell inside to the cell wall of utilizing the heat shock of vacuum microwave to get good broken wall effect to the hericium erinaceus, effectively improved the extraction rate of hericium erinaceus polysaccharide, improved the utilization ratio to the hericium erinaceus.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described above, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. The efficient extraction process of the hericium erinaceus polysaccharide is characterized by comprising the following steps of:
(1) soaking Hericium erinaceus powder in clear water to make Hericium erinaceus cells fully absorb water to obtain imbibition Hericium erinaceus powder;
(2) steaming the imbibed hericium erinaceus powder in a heating and pressurizing environment by using carbon dioxide and water vapor to obtain pretreated hericium erinaceus powder;
(3) freezing the pretreated hericium erinaceus powder to freeze liquid water absorbed in hericium erinaceus cells; then performing heat shock treatment on the frozen hericium erinaceus powder by microwaves under a vacuum condition to obtain wall-broken hericium erinaceus powder;
(4) extracting the wall-broken hericium erinaceus powder with hot water, and performing separation and purification procedures to obtain the hericium erinaceus polysaccharide extract.
2. The efficient extraction process of the hericium erinaceus polysaccharide as claimed in claim 1, wherein in the step (1), the soaking is not less than 2 hours, preferably 3-3.5 hours, and more preferably, the soaking is performed by using low-temperature water with the temperature not higher than 5 ℃.
3. The hericium erinaceus polysaccharide high-efficiency extraction process according to claim 1, wherein in the step (2), the volume ratio of the carbon dioxide to the water vapor in the step (2) is 1: 1.7-2.5, wherein the ratio of the imbibition hericium erinaceus powder to the gas is 1 g: 50-80 ml, wherein the gas is the sum of carbon dioxide and water vapor.
4. The efficient extraction process of the hericium erinaceus polysaccharide as claimed in claim 1, wherein in the step (2), the heating temperature is 105-110 ℃.
5. The efficient extraction process of the hericium erinaceus polysaccharide according to claim 1, characterized in that in the step (2), the steam curing time is 25-40 min.
6. The efficient extraction process of the hericium erinaceus polysaccharide as claimed in claim 1, wherein in the step (3), the pretreated hericium erinaceus powder is frozen to a temperature of between-10 ℃ and-15 ℃.
7. The efficient extraction process of the hericium erinaceus polysaccharide as claimed in claim 1, wherein in the step (3), the temperature of the microwave thermal shock treatment is 50-70 ℃, the time is 3-5 min, and the vacuum degree is-0.2-0.1 MPa.
8. The efficient extraction process of the hericium erinaceus polysaccharide as claimed in claim 1, wherein in the step (4), the hot water leaching temperature is 50-65 ℃, and the leaching time is 45-60 min.
9. The process for efficiently extracting the hericium erinaceus polysaccharides according to any one of claims 1 to 8, wherein in the step (4), the separation and purification process comprises: and (4) sequentially carrying out decoloring, alcohol precipitation, solid-liquid separation and vacuum drying on the leaching solution.
10. The high-efficiency extraction process of the hericium erinaceus polysaccharide as claimed in claim 9, wherein the decolorization treatment is realized by any one of activated carbon and hydrogen peroxide; preferably, the alcohol precipitation treatment is realized by using ethanol with the concentration of more than 95% and more than four times the volume of the obtained leaching liquor after decolorization, the polysaccharide is separated out in a precipitation form after the ethanol is added into the leaching liquor, and the precipitate is dried in vacuum at 40-50 ℃ after solid-liquid separation to obtain the hericium erinaceus polysaccharide extract.
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